# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2156 data_global _publ_contact_author 'Andrei S.Batsanov' _publ_contact_author_email a.s.batsanov@durham.ac.uk loop_ _publ_author_name 'Batsanov, Andrei S.' 'Eva, Pauline A.' 'Fox, Mark A.' 'Howard, Judith A. K.' 'Hughes, Andrew K.' 'Johnson, Andrew L.' 'Martin, Aileen M.' 'Wade, Ken' _journal_name_full 'Journal of the Chemical Society, Dalton Transactions' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '2000' _ccdc_journal_depnumber '?' _publ_section_title ; First structural characterisation of a 2,1,12-MC~2~B~9~ metallacarborane, [2,2,2-(NMe~2~)~3~-closo-2,1,12-TaC~2~B~9~H~11~]. Trends in boron NMR shifts on replacing a {BH} vertex with a metal {ML~n~} vertex in icosahedral carboranes. ; #====================================================================== data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2,2-tris(dimethylamido)-closo-2,1,12-tantalacarborane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H29 B9 N3 Ta' _chemical_formula_weight 445.58 _ccdc_compound_id '1' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_disorder ; none ; _ccdc_comments '?' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ta' 'Ta' -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.758(1) _cell_length_b 17.658(3) _cell_length_c 10.326(1) _cell_angle_alpha 90.00 _cell_angle_beta 96.04(1) _cell_angle_gamma 90.00 _cell_volume 1769.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 943 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 27.8 _exptl_crystal_description 'rhombohedral block' _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 6.201 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2249 _exptl_absorpt_correction_T_max 0.3693 _exptl_absorpt_process_details 'XPREP (SHELXTL, 1997); before correction R(int' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 -1.00 -1.00 0.1100 0.00 1.00 1.00 0.1100 1.00 0.00 -1.00 0.1300 -1.00 0.00 1.00 0.1300 0.00 1.00 0.00 0.1200 0.00 -1.00 0.00 0.1200 1.00 0.00 1.00 0.1750 -1.00 0.00 -1.00 0.1750 1.00 -1.00 0.00 0.1600 -1.00 1.00 0.00 0.1600 -1.00 0.00 -2.00 0.1800 1.00 0.00 2.00 0.1800 2.00 3.00 0.00 0.1400 -2.00 -3.00 0.00 0.1400 _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 10 s), each set at different \f and/or 2\q angles, nominally covered over 3/4 of the sphere of reciprocal space. The first 50 scans were repeated at the end of data collection, comparison of 299 duplicate reflections revealed no significant crystal decay. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 17446 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 29.12 _reflns_number_total 4719 _reflns_number_gt 4071 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+1.4100P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00275(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4719 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0164 _refine_ls_wR_factor_ref 0.0366 _refine_ls_wR_factor_gt 0.0352 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta2 Ta 0.768904(8) 0.125689(5) 0.945515(8) 0.01368(4) Uani 1 1 d . . . N1 N 0.6443(2) 0.20996(10) 0.97788(18) 0.0183(4) Uani 1 1 d . . . N2 N 0.94456(19) 0.18237(11) 0.97865(18) 0.0183(4) Uani 1 1 d . . . N3 N 0.7449(2) 0.07083(11) 1.10994(18) 0.0183(4) Uani 1 1 d . . . C1 C 0.8882(2) 0.07408(13) 0.7621(2) 0.0166(4) Uani 1 1 d . . . H1 H 0.968(3) 0.0892(16) 0.779(3) 0.022(7) Uiso 1 1 d . . . B3 B 0.7636(3) 0.13639(14) 0.7089(2) 0.0179(5) Uani 1 1 d . . . H3 H 0.779(3) 0.1951(15) 0.707(3) 0.019(7) Uiso 1 1 d . . . B4 B 0.8352(3) 0.07268(16) 0.5989(2) 0.0196(5) Uani 1 1 d . . . H4 H 0.899(3) 0.0978(15) 0.528(3) 0.018(7) Uiso 1 1 d . . . B5 B 0.8760(3) -0.01253(15) 0.6876(3) 0.0194(5) Uani 1 1 d . . . H5 H 0.962(3) -0.0418(16) 0.669(3) 0.022(7) Uiso 1 1 d . . . B6 B 0.8309(3) 0.00265(14) 0.8485(2) 0.0167(5) Uani 1 1 d . . . H6 H 0.897(3) -0.0237(15) 0.921(3) 0.018(7) Uiso 1 1 d . . . B7 B 0.6064(3) 0.09850(14) 0.7519(2) 0.0155(5) Uani 1 1 d . . . H7 H 0.515(3) 0.1257(15) 0.752(3) 0.020(7) Uiso 1 1 d . . . B8 B 0.6552(3) 0.08626(15) 0.5914(2) 0.0184(5) Uani 1 1 d . . . H8 H 0.592(2) 0.1094(13) 0.507(2) 0.009(6) Uiso 1 1 d . . . B9 B 0.7246(3) -0.00653(15) 0.5789(2) 0.0188(5) Uani 1 1 d . . . H9 H 0.706(3) -0.0369(16) 0.496(3) 0.027(7) Uiso 1 1 d . . . B10 B 0.7222(3) -0.05099(14) 0.7348(3) 0.0173(5) Uani 1 1 d . . . H10 H 0.696(3) -0.1083(15) 0.742(3) 0.017(7) Uiso 1 1 d . . . B11 B 0.6488(3) 0.01373(14) 0.8416(2) 0.0149(4) Uani 1 1 d . . . H11 H 0.579(3) -0.0114(16) 0.900(3) 0.023(7) Uiso 1 1 d . . . C12 C 0.5992(2) 0.01234(12) 0.6777(2) 0.0164(4) Uani 1 1 d . . . H12 H 0.510(3) -0.0053(15) 0.651(3) 0.019(7) Uiso 1 1 d . . . C13 C 0.6760(3) 0.29080(14) 0.9805(3) 0.0292(6) Uani 1 1 d . . . H131 H 0.616(3) 0.319(2) 0.908(3) 0.043(9) Uiso 1 1 d . . . H132 H 0.769(3) 0.3008(19) 0.976(3) 0.035(9) Uiso 1 1 d . . . H133 H 0.646(3) 0.3135(18) 1.058(3) 0.035(8) Uiso 1 1 d . . . C14 C 0.4972(3) 0.19792(16) 0.9915(3) 0.0269(5) Uani 1 1 d . . . H141 H 0.474(3) 0.2215(18) 1.071(3) 0.037(9) Uiso 1 1 d . . . H142 H 0.476(3) 0.1460(17) 0.991(3) 0.024(7) Uiso 1 1 d . . . H143 H 0.438(3) 0.2175(19) 0.916(3) 0.039(9) Uiso 1 1 d . . . C15 C 1.0396(3) 0.21527(16) 0.8933(3) 0.0285(6) Uani 1 1 d . . . H151 H 1.055(3) 0.2723(19) 0.911(3) 0.039(9) Uiso 1 1 d . . . H152 H 1.011(3) 0.2125(18) 0.806(3) 0.035(8) Uiso 1 1 d . . . H153 H 1.131(3) 0.1905(18) 0.906(3) 0.035(9) Uiso 1 1 d . . . C16 C 1.0001(3) 0.19671(16) 1.1153(2) 0.0258(5) Uani 1 1 d . . . H161 H 1.097(3) 0.1772(18) 1.132(3) 0.032(8) Uiso 1 1 d . . . H162 H 0.950(3) 0.1739(19) 1.175(3) 0.034(8) Uiso 1 1 d . . . H163 H 1.002(3) 0.249(2) 1.133(3) 0.039(9) Uiso 1 1 d . . . C17 C 0.7460(3) -0.00987(14) 1.1462(2) 0.0208(4) Uani 1 1 d . . . H171 H 0.809(3) -0.0171(17) 1.232(3) 0.032(8) Uiso 1 1 d . . . H172 H 0.774(3) -0.0411(18) 1.082(3) 0.031(8) Uiso 1 1 d . . . H173 H 0.654(3) -0.0255(17) 1.165(3) 0.030(8) Uiso 1 1 d . . . C18 C 0.7075(3) 0.11348(15) 1.2245(2) 0.0252(5) Uani 1 1 d . . . H181 H 0.609(3) 0.0983(16) 1.242(3) 0.023(7) Uiso 1 1 d . . . H182 H 0.710(3) 0.1716(17) 1.217(3) 0.024(7) Uiso 1 1 d . . . H183 H 0.765(3) 0.1018(15) 1.306(3) 0.022(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta2 0.01630(5) 0.01206(5) 0.01284(5) -0.00126(3) 0.00236(3) -0.00109(3) N1 0.0239(10) 0.0137(9) 0.0179(9) -0.0011(7) 0.0051(7) 0.0021(7) N2 0.0190(9) 0.0168(9) 0.0192(9) -0.0025(7) 0.0018(7) -0.0041(7) N3 0.0208(9) 0.0186(9) 0.0156(9) 0.0000(7) 0.0020(7) -0.0008(7) C1 0.0134(10) 0.0189(11) 0.0180(10) -0.0052(8) 0.0033(8) -0.0014(8) B3 0.0232(12) 0.0140(12) 0.0167(11) 0.0001(9) 0.0038(9) -0.0028(9) B4 0.0217(12) 0.0222(12) 0.0155(11) -0.0020(9) 0.0045(9) -0.0031(10) B5 0.0174(12) 0.0194(12) 0.0212(12) -0.0063(10) 0.0015(9) 0.0018(10) B6 0.0176(12) 0.0155(11) 0.0165(11) -0.0030(9) -0.0006(9) 0.0028(9) B7 0.0152(11) 0.0153(11) 0.0157(11) 0.0017(9) 0.0001(9) 0.0007(9) B8 0.0230(12) 0.0170(12) 0.0152(11) -0.0009(9) 0.0025(9) -0.0008(10) B9 0.0204(12) 0.0190(12) 0.0172(12) -0.0037(9) 0.0027(9) 0.0001(10) B10 0.0190(11) 0.0129(11) 0.0197(11) -0.0028(9) 0.0006(9) 0.0002(9) B11 0.0167(11) 0.0135(11) 0.0141(11) 0.0000(8) 0.0005(8) -0.0001(9) C12 0.0173(10) 0.0168(10) 0.0146(10) -0.0010(8) -0.0004(8) -0.0006(8) C13 0.0374(15) 0.0160(11) 0.0355(15) 0.0016(10) 0.0093(12) 0.0032(11) C14 0.0259(13) 0.0264(13) 0.0297(13) -0.0041(10) 0.0095(10) 0.0039(10) C15 0.0314(14) 0.0283(14) 0.0266(13) -0.0032(10) 0.0070(11) -0.0146(11) C16 0.0323(14) 0.0245(13) 0.0196(11) -0.0032(9) -0.0021(10) -0.0100(11) C17 0.0219(11) 0.0204(11) 0.0199(11) 0.0046(9) 0.0016(9) -0.0003(9) C18 0.0360(14) 0.0260(14) 0.0139(10) -0.0011(9) 0.0036(9) -0.0035(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta2 N1 1.9724(19) . ? Ta2 N2 1.9832(19) . ? Ta2 N3 1.9899(19) . ? Ta2 B3 2.446(3) . ? Ta2 B7 2.465(2) . ? Ta2 B11 2.484(2) . ? Ta2 B6 2.494(2) . ? Ta2 C1 2.497(2) . ? N1 C13 1.460(3) . ? N1 C14 1.472(3) . ? N2 C15 1.465(3) . ? N2 C16 1.479(3) . ? N3 C17 1.473(3) . ? N3 C18 1.480(3) . ? C1 B6 1.674(4) . ? C1 B3 1.688(3) . ? C1 B4 1.710(3) . ? C1 B5 1.711(3) . ? B3 B8 1.762(4) . ? B3 B7 1.772(4) . ? B3 B4 1.792(4) . ? B4 B9 1.766(4) . ? B4 B8 1.766(4) . ? B4 B5 1.784(4) . ? B5 B9 1.762(4) . ? B5 B10 1.763(4) . ? B5 B6 1.784(4) . ? B6 B10 1.772(4) . ? B6 B11 1.782(4) . ? B7 C12 1.702(3) . ? B7 B8 1.785(4) . ? B7 B11 1.786(3) . ? B8 C12 1.703(3) . ? B8 B9 1.783(4) . ? B9 C12 1.706(3) . ? B9 B10 1.793(4) . ? B10 C12 1.699(3) . ? B10 B11 1.789(4) . ? B11 C12 1.711(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ta2 N2 97.31(8) . . ? N1 Ta2 N3 95.31(8) . . ? N2 Ta2 N3 106.01(8) . . ? N1 Ta2 B3 99.35(8) . . ? N2 Ta2 B3 93.46(8) . . ? N3 Ta2 B3 153.89(8) . . ? N1 Ta2 B7 85.93(8) . . ? N2 Ta2 B7 135.13(8) . . ? N3 Ta2 B7 118.29(8) . . ? B3 Ta2 B7 42.31(8) . . ? N1 Ta2 B11 113.73(8) . . ? N2 Ta2 B11 146.74(8) . . ? N3 Ta2 B11 83.59(8) . . ? B3 Ta2 B11 70.77(8) . . ? B7 Ta2 B11 42.31(8) . . ? N1 Ta2 B6 154.88(8) . . ? N2 Ta2 B6 105.49(8) . . ? N3 Ta2 B6 88.51(8) . . ? B3 Ta2 B6 69.29(8) . . ? B7 Ta2 B6 70.54(8) . . ? B11 Ta2 B6 41.95(8) . . ? N1 Ta2 C1 138.49(8) . . ? N2 Ta2 C1 81.46(8) . . ? N3 Ta2 C1 125.14(8) . . ? B3 Ta2 C1 39.93(8) . . ? B7 Ta2 C1 67.99(8) . . ? B11 Ta2 C1 67.57(8) . . ? B6 Ta2 C1 39.21(8) . . ? C13 N1 C14 110.2(2) . . ? C13 N1 Ta2 127.40(17) . . ? C14 N1 Ta2 122.14(16) . . ? C15 N2 C16 108.32(19) . . ? C15 N2 Ta2 133.36(16) . . ? C16 N2 Ta2 118.32(16) . . ? C17 N3 C18 106.57(19) . . ? C17 N3 Ta2 133.58(16) . . ? C18 N3 Ta2 119.68(15) . . ? B6 C1 B3 113.26(18) . . ? B6 C1 B4 115.51(18) . . ? B3 C1 B4 63.64(15) . . ? B6 C1 B5 63.58(15) . . ? B3 C1 B5 114.98(18) . . ? B4 C1 B5 62.87(15) . . ? B6 C1 Ta2 70.28(11) . . ? B3 C1 Ta2 68.39(11) . . ? B4 C1 Ta2 129.48(15) . . ? B5 C1 Ta2 130.66(15) . . ? C1 B3 B8 104.86(17) . . ? C1 B3 B7 106.57(17) . . ? B8 B3 B7 60.66(15) . . ? C1 B3 B4 58.78(14) . . ? B8 B3 B4 59.60(15) . . ? B7 B3 B4 109.10(18) . . ? C1 B3 Ta2 71.68(11) . . ? B8 B3 Ta2 126.67(15) . . ? B7 B3 Ta2 69.42(12) . . ? B4 B3 Ta2 128.03(15) . . ? C1 B4 B9 104.16(18) . . ? C1 B4 B8 103.73(18) . . ? B9 B4 B8 60.63(15) . . ? C1 B4 B5 58.58(14) . . ? B9 B4 B5 59.51(15) . . ? B8 B4 B5 107.70(18) . . ? C1 B4 B3 57.58(14) . . ? B9 B4 B3 107.29(18) . . ? B8 B4 B3 59.35(15) . . ? B5 B4 B3 106.56(18) . . ? C1 B5 B9 104.30(18) . . ? C1 B5 B10 103.94(18) . . ? B9 B5 B10 61.17(15) . . ? C1 B5 B6 57.22(14) . . ? B9 B5 B6 108.17(18) . . ? B10 B5 B6 59.96(15) . . ? C1 B5 B4 58.55(14) . . ? B9 B5 B4 59.72(15) . . ? B10 B5 B4 108.44(18) . . ? B6 B5 B4 106.72(18) . . ? C1 B6 B10 105.07(17) . . ? C1 B6 B11 106.47(17) . . ? B10 B6 B11 60.46(14) . . ? C1 B6 B5 59.21(14) . . ? B10 B6 B5 59.43(14) . . ? B11 B6 B5 108.79(17) . . ? C1 B6 Ta2 70.51(11) . . ? B10 B6 Ta2 125.32(15) . . ? B11 B6 Ta2 68.73(11) . . ? B5 B6 Ta2 126.83(15) . . ? C12 B7 B3 102.76(17) . . ? C12 B7 B8 58.41(14) . . ? B3 B7 B8 59.39(14) . . ? C12 B7 B11 58.70(13) . . ? B3 B7 B11 106.68(17) . . ? B8 B7 B11 108.08(18) . . ? C12 B7 Ta2 122.14(14) . . ? B3 B7 Ta2 68.27(11) . . ? B8 B7 Ta2 124.41(15) . . ? B11 B7 Ta2 69.41(11) . . ? C12 B8 B3 103.14(17) . . ? C12 B8 B4 104.21(18) . . ? B3 B8 B4 61.04(15) . . ? C12 B8 B9 58.57(14) . . ? B3 B8 B9 107.86(18) . . ? B4 B8 B9 59.67(15) . . ? C12 B8 B7 58.36(14) . . ? B3 B8 B7 59.95(14) . . ? B4 B8 B7 109.69(17) . . ? B9 B8 B7 108.61(18) . . ? C12 B9 B5 103.70(17) . . ? C12 B9 B4 104.08(18) . . ? B5 B9 B4 60.77(15) . . ? C12 B9 B8 58.37(14) . . ? B5 B9 B8 107.96(18) . . ? B4 B9 B8 59.71(15) . . ? C12 B9 B10 58.04(14) . . ? B5 B9 B10 59.44(15) . . ? B4 B9 B10 107.90(18) . . ? B8 B9 B10 107.23(17) . . ? C12 B10 B5 103.97(18) . . ? C12 B10 B6 103.29(17) . . ? B5 B10 B6 60.61(15) . . ? C12 B10 B11 58.68(13) . . ? B5 B10 B11 109.39(18) . . ? B6 B10 B11 60.03(14) . . ? C12 B10 B9 58.42(14) . . ? B5 B10 B9 59.40(15) . . ? B6 B10 B9 107.29(18) . . ? B11 B10 B9 108.54(18) . . ? C12 B11 B6 102.41(17) . . ? C12 B11 B7 58.18(13) . . ? B6 B11 B7 106.75(17) . . ? C12 B11 B10 58.04(14) . . ? B6 B11 B10 59.51(14) . . ? B7 B11 B10 107.52(17) . . ? C12 B11 Ta2 120.68(14) . . ? B6 B11 Ta2 69.32(11) . . ? B7 B11 Ta2 68.28(11) . . ? B10 B11 Ta2 125.00(15) . . ? B10 C12 B7 115.97(17) . . ? B10 C12 B8 115.60(18) . . ? B7 C12 B8 63.23(14) . . ? B10 C12 B9 63.54(15) . . ? B7 C12 B9 116.45(18) . . ? B8 C12 B9 63.06(15) . . ? B10 C12 B11 63.29(14) . . ? B7 C12 B11 63.11(14) . . ? B8 C12 B11 115.70(17) . . ? B9 C12 B11 116.63(18) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.12 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.885 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.083 #==================================================END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2,2-tris(dimethylamido)-closo-2,1,7-tantalacarborane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H29 B9 N3 Ta' _chemical_formula_weight 445.58 _ccdc_compound_id '2' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_disorder ; All three NMe~2~ groups, i.e. the atoms N(1), N(2), N(3), C(13) to C(18) with their hydrogens, are disordered between two sets of positions, related by the crystallographic mirror plane. ; _ccdc_comments '?' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ta' 'Ta' -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 10.538(1) _cell_length_b 12.001(1) _cell_length_c 14.136(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1787.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 986 _cell_measurement_theta_min 12 _cell_measurement_theta_max 23 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 6.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2341 _exptl_absorpt_correction_T_max 0.3568 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998), R(int)=0.144 before correction' _exptl_special_details ; The data collection nominally covered ca. 3/4 of the sphere of reciprocal space, by a combination of 4 sets of \w scans; each set at different \f and/or 2\q angles and each scan (15 sec exposure) covering 0.3\% in \w. Crystal decay was monitored by repeating 50 initial frames at the end of data collection and comparing duplicate reflections. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 _diffrn_reflns_number 16808 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 29.17 _reflns_number_total 2517 _reflns_number_gt 2353 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+42.6501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2517 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_restrained_S_all 1.320 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta2 Ta 0.21579(4) 0.2500 0.43065(3) 0.01676(15) Uani 1 2 d S . . C1 C 0.3950(7) 0.1388(7) 0.4970(6) 0.0178(14) Uani 1 1 d . . . H1 H 0.3829 0.0571 0.4599 0.027 Uiso 1 1 d R . . B3 B 0.2931(8) 0.1752(8) 0.5840(6) 0.0188(16) Uani 1 1 d . . . H3 H 0.2115 0.1239 0.6103 0.028 Uiso 1 1 d R . . B4 B 0.4510(8) 0.1302(8) 0.6101(7) 0.0208(18) Uani 1 1 d . . . H4 H 0.4694 0.0501 0.6482 0.031 Uiso 1 1 d R . . B5 B 0.5502(8) 0.1770(8) 0.5156(7) 0.0183(16) Uani 1 1 d . . . H5 H 0.6348 0.1280 0.4916 0.027 Uiso 1 1 d R . . B6 B 0.4478(11) 0.2500 0.4367(9) 0.017(2) Uani 1 2 d S . . H6 H 0.4687 0.2500 0.3590 0.025 Uiso 1 2 d SR . . B7 B 0.3881(12) 0.2500 0.6670(9) 0.022(3) Uani 1 2 d S . . H7 H 0.3661 0.2500 0.7445 0.032 Uiso 1 2 d SR . . B8 B 0.5500(11) 0.2500 0.6245(9) 0.018(2) Uani 1 2 d S . . H8 H 0.6342 0.2500 0.6729 0.028 Uiso 1 2 d SR . . N1 N 0.0447(13) 0.2151(11) 0.4823(10) 0.023(3) Uiso 0.50 1 d P . . N2 N 0.2109(14) 0.1385(13) 0.3262(11) 0.021(3) Uiso 0.50 1 d P . . N3 N 0.1755(14) 0.3819(13) 0.3625(11) 0.022(3) Uiso 0.50 1 d P . . C13 C -0.0060(16) 0.2240(13) 0.5795(11) 0.027(4) Uiso 0.50 1 d P . . H131 H -0.0936 0.2019 0.5803 0.040 Uiso 0.50 1 d PR . . H132 H 0.0422 0.1754 0.6197 0.040 Uiso 0.50 1 d PR . . H133 H 0.0013 0.2992 0.6020 0.040 Uiso 0.50 1 d PR . . C14 C -0.0507(16) 0.159(2) 0.4224(15) 0.042(6) Uani 0.50 1 d P . . H141 H -0.1268 0.1498 0.4589 0.064 Uiso 0.50 1 d PR . . H142 H -0.0681 0.2053 0.3686 0.064 Uiso 0.50 1 d PR . . H143 H -0.0212 0.0875 0.4014 0.064 Uiso 0.50 1 d PR . . C15 C 0.2206(19) 0.0149(17) 0.3373(14) 0.030(4) Uiso 0.50 1 d P . . H151 H 0.2160 -0.0192 0.2760 0.045 Uiso 0.50 1 d PR . . H152 H 0.2994 -0.0049 0.3670 0.045 Uiso 0.50 1 d PR . . H153 H 0.1512 -0.0107 0.3755 0.045 Uiso 0.50 1 d PR . . C16 C 0.2143(17) 0.1658(19) 0.2255(13) 0.032(4) Uani 0.50 1 d P . . H161 H 0.2107 0.0997 0.1872 0.048 Uiso 0.50 1 d PR . . H162 H 0.1434 0.2129 0.2106 0.048 Uiso 0.50 1 d PR . . H163 H 0.2919 0.2049 0.2129 0.048 Uiso 0.50 1 d PR . . C17 C 0.2645(18) 0.4501(17) 0.3043(14) 0.029(4) Uiso 0.50 1 d P . . H171 H 0.2208 0.5118 0.2759 0.044 Uiso 0.50 1 d PR . . H172 H 0.3290 0.4775 0.3463 0.044 Uiso 0.50 1 d PR . . H173 H 0.3030 0.4055 0.2558 0.044 Uiso 0.50 1 d PR . . C18 C 0.0540(19) 0.442(2) 0.366(2) 0.050(7) Uani 0.50 1 d P . . H181 H 0.0521 0.5060 0.3251 0.075 Uiso 0.50 1 d PR . . H182 H -0.0147 0.3932 0.3504 0.075 Uiso 0.50 1 d PR . . H183 H 0.0455 0.4663 0.4306 0.075 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta2 0.0114(2) 0.0210(2) 0.0178(2) 0.000 -0.00097(16) 0.000 C1 0.015(3) 0.020(4) 0.019(3) 0.002(3) -0.001(3) 0.000(3) B3 0.015(3) 0.026(4) 0.016(4) 0.003(3) -0.002(3) 0.001(3) B4 0.017(4) 0.022(4) 0.023(4) 0.006(4) -0.001(3) 0.000(3) B5 0.012(3) 0.020(4) 0.023(4) -0.002(3) 0.000(3) 0.001(3) B6 0.016(5) 0.013(5) 0.020(6) 0.000 0.003(5) 0.000 B7 0.017(6) 0.031(7) 0.016(6) 0.000 -0.003(5) 0.000 B8 0.013(5) 0.023(6) 0.019(6) 0.000 -0.001(4) 0.000 C14 0.012(7) 0.083(17) 0.032(10) -0.014(11) -0.002(7) -0.010(9) C16 0.022(8) 0.047(12) 0.026(9) 0.006(8) 0.001(7) 0.006(8) C18 0.025(9) 0.049(14) 0.076(17) 0.038(13) 0.007(10) 0.010(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta2 N3 1.902(15) . ? Ta2 N1 1.990(14) . ? Ta2 N2 1.994(15) . ? Ta2 B6 2.447(12) . ? Ta2 B3 2.484(9) . ? Ta2 C1 2.495(8) . ? C1 B6 1.678(11) . ? C1 B3 1.691(12) . ? C1 B4 1.709(12) . ? C1 B5 1.719(12) . ? B3 B7 1.785(14) . ? B3 B4 1.788(13) . ? B3 B3 1.80(2) 7_565 ? B4 B7 1.775(13) . ? B4 B5 1.787(13) . ? B4 B8 1.787(12) . ? B5 B5 1.752(19) 7_565 ? B5 B8 1.771(15) . ? B5 B6 1.782(15) . ? B7 B8 1.808(18) . ? N1 C14 1.48(2) . ? N1 C13 1.48(2) . ? N2 C16 1.46(2) . ? N2 C15 1.50(2) . ? N3 C18 1.47(2) . ? N3 C17 1.49(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ta2 N1 99.2(6) . . ? N3 Ta2 N2 100.2(7) . . ? N1 Ta2 N2 96.2(6) . . ? N3 Ta2 B6 103.9(5) . . ? N1 Ta2 B6 153.2(5) . . ? N2 Ta2 B6 93.0(5) . . ? N3 Ta2 B3 144.8(5) . . ? N1 Ta2 B3 84.3(5) . . ? N2 Ta2 B3 114.3(5) . . ? B6 Ta2 B3 69.0(3) . . ? B3 Ta2 B3 42.4(5) 7_565 . ? B6 Ta2 C1 39.7(3) . 7_565 ? N3 Ta2 C1 143.6(5) . . ? N1 Ta2 C1 115.8(4) . . ? N2 Ta2 C1 86.5(5) . . ? B6 Ta2 C1 39.7(3) . . ? B3 Ta2 C1 67.5(3) 7_565 . ? B3 Ta2 C1 39.7(3) . . ? C1 Ta2 C1 64.7(4) 7_565 . ? B6 C1 B3 112.1(7) . . ? B6 C1 B4 114.1(7) . . ? B3 C1 B4 63.5(5) . . ? B6 C1 B5 63.2(6) . . ? B3 C1 B5 115.1(6) . . ? B4 C1 B5 62.8(5) . . ? B6 C1 Ta2 68.6(5) . . ? B3 C1 Ta2 69.8(4) . . ? B4 C1 Ta2 130.2(5) . . ? B5 C1 Ta2 129.4(5) . . ? C1 B3 B7 104.6(7) . . ? C1 B3 B4 58.8(5) . . ? B7 B3 B4 59.6(5) . . ? C1 B3 B3 104.9(4) . 7_565 ? B7 B3 B3 59.8(4) . 7_565 ? B4 B3 B3 107.5(4) . 7_565 ? C1 B3 Ta2 70.5(4) . . ? B7 B3 Ta2 125.1(5) . . ? B4 B3 Ta2 126.5(5) . . ? B3 B3 Ta2 68.8(2) 7_565 . ? C1 B4 B7 104.2(7) . . ? C1 B4 B5 58.9(5) . . ? B7 B4 B5 107.6(7) . . ? C1 B4 B8 105.1(7) . . ? B7 B4 B8 61.0(6) . . ? B5 B4 B8 59.4(6) . . ? C1 B4 B3 57.8(5) . . ? B7 B4 B3 60.1(6) . . ? B5 B4 B3 107.2(6) . . ? B8 B4 B3 108.9(7) . . ? C1 B5 B5 105.5(4) . 7_565 ? C1 B5 B8 105.3(7) . . ? B5 B5 B8 60.4(4) 7_565 . ? C1 B5 B4 58.3(5) . . ? B5 B5 B4 108.3(4) 7_565 . ? B8 B5 B4 60.3(5) . . ? C1 B5 B6 57.2(5) . . ? B5 B5 B6 60.6(4) 7_565 . ? B8 B5 B6 107.5(6) . . ? B4 B5 B6 105.6(6) . . ? C1 B6 C1 105.3(9) . 7_565 ? C1 B6 B5 105.9(8) . 7_565 ? C1 B6 B5 59.5(5) 7_565 7_565 ? C1 B6 B5 59.5(5) . . ? B5 B6 B5 58.9(7) 7_565 . ? C1 B6 Ta2 71.7(5) . . ? B5 B6 Ta2 128.8(6) . . ? B4 B7 B4 108.1(9) . 7_565 ? B4 B7 B3 60.3(5) . . ? B4 B7 B3 108.7(8) 7_565 . ? B4 B7 B3 60.3(5) 7_565 7_565 ? B3 B7 B3 60.4(7) . 7_565 ? B4 B7 B8 59.8(5) . . ? B4 B7 B8 59.8(5) 7_565 . ? B3 B7 B8 108.1(8) . . ? B5 B8 B5 59.3(7) . 7_565 ? B5 B8 B4 60.3(5) . . ? B5 B8 B4 107.4(8) 7_565 . ? B4 B8 B4 107.1(9) . 7_565 ? B5 B8 B7 106.9(7) . . ? B4 B8 B7 59.2(5) . . ? C14 N1 C13 108.6(13) . . ? C14 N1 Ta2 120.1(11) . . ? C13 N1 Ta2 130.8(11) . . ? C16 N2 C15 108.8(15) . . ? C16 N2 Ta2 124.8(13) . . ? C15 N2 Ta2 125.9(12) . . ? C18 N3 C17 107.2(15) . . ? C18 N3 Ta2 125.9(13) . . ? C17 N3 Ta2 126.5(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.17 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 4.282 _refine_diff_density_min -5.977 _refine_diff_density_rms 0.289 #===================================================END